CN101186569A - Continuous co-production method for high concentration formic acid and high pure sodium hexametaphosphate - Google Patents
Continuous co-production method for high concentration formic acid and high pure sodium hexametaphosphate Download PDFInfo
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- CN101186569A CN101186569A CNA2007100780732A CN200710078073A CN101186569A CN 101186569 A CN101186569 A CN 101186569A CN A2007100780732 A CNA2007100780732 A CN A2007100780732A CN 200710078073 A CN200710078073 A CN 200710078073A CN 101186569 A CN101186569 A CN 101186569A
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Abstract
The invention relates to a continuous preparation method of concentrated formic acid with joint production of high pure hexametaphosphate, which comprises arranging peroxyphosphoric acid and sodium formate simultaneously into a cone-type mixer to be mixed uniformly and reacted instantly, while the generated formic acid presses the generated mixed materials into a distillation drier to be distilled and dried into dry powder of composite phosphate, feeding the generated formic acid gas into a washing dewatering purifier to be washed, purified and dewatered via peroxyphosphoric acid to be fed into a condenser to separate formic acid, controlling the condensation temperature to obtain concentrated formic acid, pumping out the foul gas under vacuum, automatically discharging the generated dry powder of composite phosphate automatically out from the distillation drier to be directly fed into a polyfurnace or first prepared into solution to be fed into a polyfurnace, continuously adding industrial phosphoric acid, and obtaining high pure hexametaphosphate. The invention has high production efficiency, reduced acidification reactor, continuous operation, large production capacity, non formic acid gas leakage in process, improved workshop environment, high product yield, high formic acid density, better economic and environment benefits.
Description
Technical field
The present invention relates to aliphatic carboxylic acid and alkali metal phosphate, in particular to the preparation method of formic acid and sodium phosphate salt.
Background technology
Produce the method for formic acid and coproduction Sodium hexametaphosphate 99, had the ZL97103209.2 patent to make public.Yet this method has the following disadvantages: the one, and technical process is discontinuous, all intermittently finishes with peroxophosphoric acid acidifying sodium formate, each operation of producing formic acid; The 2nd, acidizing process need be set, and raw material peroxophosphoric acid and sodium formiate must feed intake successively during acidifying, the batch mixing under stirring through about 15min reacts and just can enter distillation process; The 3rd, discharging a large amount of reaction heat owing to acidification reaction, formic acid gas overflows contaminate environment, even if adopt measures such as chuck cooling, vacuum absorption, effect is unsatisfactory; The 4th, the formic acid yield is low, whole process of production needs 2～2.5h consuming time, and production efficiency is low; The 5th, the formic acid concn majority that makes has only 85%, does not go because of the moisture in the formic acid gas that distills out to remove, so the concentration formic acid and high that obtains seldom, its added value is also just carried not high.
Summary of the invention
Purpose of the present invention is exactly the shortcoming that exists at prior art, provide a kind of serialization to produce the method for the high-purity Sodium hexametaphosphate 99 of concentration formic acid and high coproduction, improve the production efficiency of whole process, the concentration and the yield of formic acid, thereby improve added value of product, create better economic benefit.
The contriver is through years of researches and test, and the novel method that provides comprises following operation:
At first, peroxophosphoric acid and sodium formiate are dropped into cone mixer simultaneously, both promptly react by the moment mixing, and the pressure that the formic acid gas of generation forms just is pressed into the distillation moisture eliminator with the mixture that generates, and make composite phosphate dry powder after the distillation drying; The formic acid gas that produces then enters subsequent processing;
The formic acid gas that last operation produces enters the washing dehydration cleaner, the peroxophosphoric acid with 105%～115% wash, purify and dewater after enter condenser, the formic acid that condensation is got off collects, and controls its processing condition and can obtain various concentration formic acid and highs; Non-condensable gases is then extracted out with vacuum;
The composite phosphate dry powder that first operation produces flows out automatically from the distillation moisture eliminator, directly be mixed with solution with dry powder or with clear water, through mending acid for adjusting pH value, the polycondensation by routine promptly makes high-purity Sodium hexametaphosphate 99, or Trisodium trimetaphosphate, or SODIUM PHOSPHATE, MONOBASIC etc.; Or regulate the pH value through adding alkali, the polycondensation by routine promptly makes tripoly phosphate sodium STPP, or trisodium phosphate, or Sodium phosphate dibasic, or tertiary sodium phosphate etc.
Peroxophosphoric acid is with P described in aforesaid method first operation
2O
5The concentration of meter is 76%～83%; The purity of described sodium formiate 〉=95%.
The described distillation moisture eliminator of first operation is commercially available two blade distillation drying machines in the aforesaid method.
The described various concentration formic acid and highs of second operation in the aforesaid method are that content is 90%～98% formic acid, also can make 85% formic acid according to customer requirements.
The described solution of the 3rd operation is to be 40%～50% solution at 〉=100 ℃ of following compound concentrations in the aforesaid method.
The present invention has following advantage: 1. production efficiency height, from being dosed into out composite phosphate dry powder, only need 60～80min, and the time spent shortens more than 1/3 than original technology; 2. reduced the acidifying still of original technology, system moves continuously, and sodium formiate and peroxophosphoric acid feed intake simultaneously, produces formic acid and composite phosphate dry powder continuously; The throughput of equipment is scalable, and single cover output can improve 5 times; 3. there be not overflowing of formic acid gas in the process, workshop air cleaning, environmental friendliness; 4. original process recovery ratio is not high, and this process recovery ratio reaches more than 95%, the formic acid concn height, and can regulate arbitrarily, increased added value of product.As seen the present invention has favorable economic benefit and environmental benefit.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment
Embodiment
Will be with P
2O
5To be 76% peroxophosphoric acid and purity drop into cone mixer for 〉=95% sodium formiate to meter concentration simultaneously, these both moment mixings promptly react, the pressure that the formic acid gas that produces forms just is pressed into the distillation moisture eliminator with the mixture that generates, and makes composite phosphate dry powder after the distillation drying; The formic acid gas that produces then enters the washing dehydration cleaner, peroxophosphoric acid with＞105% wash, purify and dewater after enter condenser, the formic acid that condensation is got off is separated, controlling its condensing temperature is 10 ℃, obtain concentration and be 96% formic acid, non-condensable gases is then extracted out with vacuum; The composite phosphate dry powder that produces flows out automatically from the distillation moisture eliminator, directly imports polymerization furnace successively, adds industrial phosphoric acid in the process continuously, makes Na
2O and P
2O
5Mol ratio be 1, make high-purity Sodium hexametaphosphate 99, its quality index is with P
2O
5Meter, total phosphate 〉=68%, nonactive phosphoric acid salt 3%.
Used mixing tank is that commercially available model is the mixing tank of RDS-0.05 in the process; Used distillation moisture eliminator is that commercially available model is the distillation moisture eliminator of JG-160; Used condenser is board-like graphite condenser.
Claims (5)
1. the method for the high-purity Sodium hexametaphosphate 99 of concentration formic acid and high coproduction is produced in a serialization, is to obtain formic acid and composite phosphate with the peroxophosphoric acid acidifying sodium formate, and its feature comprises following operation:
At first, peroxophosphoric acid and sodium formiate are dropped into cone mixer simultaneously, both promptly react by the moment mixing, and the pressure that the formic acid gas of generation forms just is pressed into the distillation moisture eliminator with the mixture that generates, and make composite phosphate dry powder after the distillation drying; The formic acid gas that produces then enters subsequent processing;
The formic acid gas that last operation produces enters the washing dehydration cleaner, the peroxophosphoric acid with＞105% wash, purify and dewater after enter condenser, the formic acid that condensation is got off is separated, control its processing condition and can obtain various concentration formic acid and highs; Non-condensable gases is then extracted out with vacuum;
The composite phosphate dry powder that first operation produces flows out automatically from the distillation moisture eliminator, directly is mixed with solution with dry powder or with clear water, and through mending acid for adjusting pH value, the polycondensation by routine promptly makes high-purity Sodium hexametaphosphate 99, or Trisodium trimetaphosphate, or SODIUM PHOSPHATE, MONOBASIC; Or regulate the pH value through adding alkali, the polycondensation by routine promptly makes tripoly phosphate sodium STPP, or trisodium phosphate, or Sodium phosphate dibasic, or tertiary sodium phosphate.
2. in accordance with the method for claim 1, it is characterized in that peroxophosphoric acid in described method first operation is with P
2O
5The concentration of meter is 76%～83%; The purity of sodium formiate 〉=95%.
3. in accordance with the method for claim 1, it is characterized in that the moisture eliminator of distillation described in described method first operation is commercially available two blade distillation drying machines.
4. in accordance with the method for claim 1, it is characterized in that the described various concentration formic acid and highs of second operation in the described method, is that content is 90%～98% formic acid, or 85% formic acid.
5. in accordance with the method for claim 1, it is characterized in that the described solution of the 3rd operation in the described method is is 40%～50% solution at 〉=100 ℃ of following compound concentrations.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100780732A CN100480227C (en) | 2007-12-28 | 2007-12-28 | Continuous co-production method for high concentration formic acid and high pure sodium hexametaphosphate |
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|---|---|---|---|
| CNB2007100780732A CN100480227C (en) | 2007-12-28 | 2007-12-28 | Continuous co-production method for high concentration formic acid and high pure sodium hexametaphosphate |
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| CN101186569A true CN101186569A (en) | 2008-05-28 |
| CN100480227C CN100480227C (en) | 2009-04-22 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362682B (en) * | 2008-09-23 | 2011-02-09 | 余华强 | Method for producing formic acid with joint production of sodium phosphate by peroxyphosphoric acid and sodium formate |
| CN101597045B (en) * | 2009-07-03 | 2011-08-31 | 贵州青利集团股份有限公司 | Method for preparing trimeric sodium phosphate by composite phosphate dry powder |
| CN101475463B (en) * | 2009-01-21 | 2011-09-21 | 曹勇 | Method for coproduction of high purity aminic acid and acid sodium phosphate by reaction of calcium formate and peroxyphosphoric acid |
| CN104788304A (en) * | 2015-03-26 | 2015-07-22 | 重庆川东化工（集团）有限公司 | Method for preparing high-purity anhydrous formic acid from inorganic acid acidification formate |
| CN106241767A (en) * | 2016-08-29 | 2016-12-21 | 武汉东晟捷能科技有限公司 | A kind of method preparing potassium dihydrogen phosphate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE309412B (en) * | 1964-04-03 | 1969-03-24 | Perstorp Ab |
-
2007
- 2007-12-28 CN CNB2007100780732A patent/CN100480227C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362682B (en) * | 2008-09-23 | 2011-02-09 | 余华强 | Method for producing formic acid with joint production of sodium phosphate by peroxyphosphoric acid and sodium formate |
| CN101475463B (en) * | 2009-01-21 | 2011-09-21 | 曹勇 | Method for coproduction of high purity aminic acid and acid sodium phosphate by reaction of calcium formate and peroxyphosphoric acid |
| CN101597045B (en) * | 2009-07-03 | 2011-08-31 | 贵州青利集团股份有限公司 | Method for preparing trimeric sodium phosphate by composite phosphate dry powder |
| CN104788304A (en) * | 2015-03-26 | 2015-07-22 | 重庆川东化工（集团）有限公司 | Method for preparing high-purity anhydrous formic acid from inorganic acid acidification formate |
| CN106241767A (en) * | 2016-08-29 | 2016-12-21 | 武汉东晟捷能科技有限公司 | A kind of method preparing potassium dihydrogen phosphate |
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|---|---|
| CN100480227C (en) | 2009-04-22 |
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